Patent GB-796544-A (GB)
Title: Improvements in the manufacture of artificial filaments and like products
Inventor: FINLAYSON DONALD
IPC: D01F2/28
Filed: 1954-10-13
Abstract: Cellulose triacetate filaments, films and like products are made by shaping, by extrusion or casting, a composition comprising a cellulose triacetate dissolved in or gelled with cyclohexanone at above 50 DEG  C., preferably above 70 DEG  C., cooling the shaped composition to below 50 DEG  C., preferably below 40 DEG  C., and simultaneously or subsequently removing cyclohexanone from the resulting shaped article, preferably by washing.  The composition preferably contains 12 per cent or more, e.g. up to about 15-20 per cent, of cellulose triacetate, and may be made by dissolving the cellulose triacetate in the cyclohexanone at about 150-155 DEG  C. under atmospheric pressure or at temperatures up to about 160-165 DEG C. at somewhat higher pressures.  The cooling medium in the setting zone may be either a gas or a liquid, and is advantageously at a temperature below 30 DEG  C. and especially 10-25 DEG  C.  In addition the filaments, films, or like products, may travel in contact with a solid surface at a similar temperature, e.g. a hollow roller through which cold water is passed.  The composition may be extruded into a liquid which is miscible with cyclohexanone but does not dissolve cellulose triacetate, e.g. a liquid hydrocarbon or an aliphatic alcohol containing up to 5 carbon atoms.  Examples include t-butyl alcohol, benzene, toluene, cyclohexane and petroleum ether of 60-80 DEG  C. boiling range.  There is preferably an air gap of about 0.25-2 inches between the face of the spinning jet and the cooling liquid.  The composition may also be extruded into water, preferably containing a surface tension-reducing agent such as Turkey Red oil, or into air, and the filamentary material so obtained may be washed with a lower aliphatic alcohol or a liquid hydrocarbon. Cyclohexanone may alternatively be removed from the extruded material by heating for a short time to about 140-160 DEG  C.  Filamentary material is preferably drawn from the spinning jet under a tension sufficient to stretch it by at least twice, and especially by about 3-10 times.  Alternatively, filaments, especially those of denier above about 10, may be extruded into a cooling liquid without the application of any tension and allowed to lie in the cooling liquid for a short time.  The filaments then generally have a high degree of crimp, irrespective of whether or not the cooling liquid is a solvent for cyclohexanone.  In an example, cellulose triacetate is dissolved in boiling cyclohexanone to give a 15 per cent solution which is formed hot into rods which are solidified by cooling.  The solid rods are urged against the internal face of a single orifice spinneret heated to 100-110 DEG  C. and the monofil so formed is drawn first through a short air gap and then through an isopropanol bath at 20 DEG  C. by a godet having a peripheral speed 8-10 times the linear speed of extrusion.  The filament is dried at 70-80 DEG  C.  In another example, a 15 per cent solution of cellulose triacetate in cyclohexanone is cooled to 75-90 DEG  C. and the resulting gel is extruded through a one-hole spinneret by means of a screw press. The monofil so produced is allowed to fall through a setting cell about 10 feet long down which a current of air at about 20 DEG  C. is drawn continuously.  After leaving the bottom of the setting cell the filament is continuously washed until free from cyclohexanone and dried.